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经衍生化后,采用气相色谱-质谱法对臭氧氧化和氯化水以及海水的溴酸盐进行灵敏测定。

Sensitive determination of bromate in ozonated and chlorinated water, and sea water by gas chromatography-mass spectrometry after derivatization.

机构信息

Department of Environmental Education, Kongju National University, Kongju 314-701, South Korea.

出版信息

J Chromatogr A. 2012 Feb 3;1223:136-41. doi: 10.1016/j.chroma.2011.12.059. Epub 2011 Dec 26.

DOI:10.1016/j.chroma.2011.12.059
PMID:22227358
Abstract

A sensitive gas chromatographic method has been established for the determination of bromate in ozonated and chlorinated water, and in sea water. With acidic conditions, bromate reacts with chloride to form bromine, which reacts with 2,6-dialkylphenol to form 4-bromo-2,6-dialkylphenol. The organic derivative was extracted with ethyl acetate after quenching remaining oxidants with ascorbic acid, and then measured by gas chromatography-mass spectrometry (GC-MS). The lowest detection limit and limit of quantification of bromate in drinking water were 0.02 and 0.07 μg/L, respectively, and the calibration curve showed good linearity with r²=0.998. The 32 common ions did not interfere even when present in 100-fold excess over the bromated ion. The accuracy was in a range of 102-106% and the precision of the assay was less than 6% in chlorinated and ozonated tap water, ozonated mineral water, and sea water. The method was sensitive, reproducible and simple enough to permit reliable analysis of bromate to the ng/L level in water.

摘要

建立了一种灵敏的气相色谱法,用于测定臭氧和氯化水中以及海水中的溴酸盐。在酸性条件下,溴酸盐与氯离子反应生成溴,溴与 2,6-二烷基苯酚反应生成 4-溴-2,6-二烷基苯酚。用抗坏血酸淬灭剩余氧化剂后,用乙酸乙酯萃取有机衍生物,然后用气相色谱-质谱法(GC-MS)进行测定。饮用水中溴酸盐的最低检测限和定量限分别为 0.02 和 0.07μg/L,校准曲线的线性良好,r²=0.998。即使存在 100 倍过量的溴酸盐离子,32 种常见离子也没有干扰。在氯化和臭氧处理的自来水、臭氧处理的矿泉水和海水中,该方法的准确度在 102-106%之间,测定的精密度小于 6%。该方法灵敏、重现性好且足够简单,可可靠地分析水中的 ng/L 水平的溴酸盐。

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